Skip to main content

Calibration and validation of microscopic X-ray fluorescence analysis for determination of heavy metals in polymers and fly-ash particles

Objective


Foreseen Results

Initially, after optimisation of the instrumentation and adaptation/installation of appropriate data processing software at the Polish and Hungarian institutes suitable for resp. trace analysis of polymer samples and individual fly-ash particulates, standardized analysis protocols for these two types of analysis will be established via the use of well-characterised materials and standards. To validate these protocols, a set of realistic polymer and fly-ash samples will be composed and the same samples will be analysed by four micro-XRF instruments and by other microanalytical methods of comparable capabilities. Comparison of the results will allow the collaborating partners to evaluate in a detailed way the strong and weak points of m-XRF in terms of accuracy, precision, sensitivity, lateral resolution and cost of analysis and will provide them with a very concrete picture on the practical usefulness of this technique in the context of (a) industrial quality assurance and compliance to regulations (polymers), (b) hazard assessment in environmental pollution problems (fly-ash and aerosols). If this project is successful, a novel and optimised technique will be available for quantitative microscopical characterisation of a variety of materials with respect to the abundance of heavy trace metals and by means of equipment which is significantly simpler in construction and price than a conventional electron microscope.
With the aim of contributing to the development of (micro-)chemical metrology and its introduction in routine analysis, the subject of the present Joint Research Project (JRP) is the calibration and validation of the microscopic X-ray fluorescence technique for the reliable quantitative determination of the distribution of heavy metals in industrial materials (various types of polymers) and in environmental particulate matter produced during industrial activities (fly-ash particles and other industrial dust).
Microscopic X-ray fluorescence analysis (m-XRF) is an energy-dispersive form of the bulk XRF technique that has been commercially available for a number of years, with a lateral resolution at the 10mm level and detection limits at the 10 ppm level relative or 1 pg absolute. Compared to electron probe X-ray microanalysis, microscopic X-ray fluorescence features a much better elemental sensitivity but is limited in lateral resolution. This combination of lateral resolution sensitivity makes m-XRF to some extent comparable to m-PIXE (proton induced X-ray emission) but requires equipment of far less cost and degree of sophistication which is within the reach of most laboratories already employing bulk XRF in its energy-dispersive form.
The quantitative capabilities of m-XRF for microscopic analysis of trace concentrations(10-100 ppm level) of heavy metals in industrial materials such as polypropylene or polyethene and in environmental samples such as individual fly-ash particles (produced during burning of fossil fuels for power generation, especially in Eastern European countries) has never been thoroughly compared to that of established microscopical and macroscopical analysis techniques.

Coordinator

N/A

Participants (5)

Chalmers University of Technology AB
Sweden
Address
1,Kemigarden 1
412 96 Göteborg
DSM Research BV
Netherlands
Address
1,
6160 MD Geleen
KFKI - Atomic Energy Research Institute - Hungarian Academy of Sciences
Hungary
Address
29-33,Konkoly-thege Ut 29-33
1525 Budapest
Thermal Comfort Ltd.
Hungary
Address
43/C,nagybanyai 43/C
1025 Budapest
University of Mining and Metallurgy
Poland
Address
30,Al. Mickiewicza 30
30 059 Kraków